CN108996487A - A kind of method that carbon nano pipe array is separated with growth substrate - Google Patents
A kind of method that carbon nano pipe array is separated with growth substrate Download PDFInfo
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- CN108996487A CN108996487A CN201710423271.1A CN201710423271A CN108996487A CN 108996487 A CN108996487 A CN 108996487A CN 201710423271 A CN201710423271 A CN 201710423271A CN 108996487 A CN108996487 A CN 108996487A
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- Prior art keywords
- pipe array
- carbon nano
- nano pipe
- substrate
- separated
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
- B01J21/185—Carbon nanotubes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0004—Apparatus specially adapted for the manufacture or treatment of nanostructural devices or systems or methods for manufacturing the same
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0009—Forming specific nanostructures
- B82B3/0014—Array or network of similar nanostructural elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The present invention relates to a kind of method that carbon nano pipe array is separated with growth substrate, specifically includes the following steps: provide all one's life with carbon nano pipe array substrate；The substrate is heated, and is passed through oxygen or oxygenous mixed gas, reacts the carbon nano pipe array with oxygen；Separate the carbon nano pipe array and substrate.
Description
Technical field
The present invention relates to a kind of methods that carbon nano pipe array is separated with growth substrate.
Background technique
Carbon nanotube is a kind of new one-dimensional nano material just found the early 1990s.The special construction of carbon nanotube is determined
It has been determined with special property, such as high-tensile and high thermal stability；With the variation of carbon nanotube spiral way, carbon is received
Mitron can show metallicity or semiconductive etc..Due to carbon nanotube have ideal one-dimentional structure and mechanics, electricity,
The excellent property in the fields such as calorifics, wide application has been shown in interdisciplinary fields such as material science, chemistry, physics
Prospect is also received more and more attention in scientific research and industry using upper.
The method of the preparation carbon nanotube of comparative maturity mainly includes arc discharge method (Arc discharge), swashs at present
Light ablation (Laser Ablation) and chemical vapour deposition technique (Chemical Vapor Deposition).Wherein, chemical
Vapour deposition process and first two method, which are compared, has that yield is high, controllability is strong, mutually compatible with existing integrated circuit technology etc. excellent
Point convenient for industrially being synthesized on a large scale, therefore was concerned in recent years.
After growing carbon nano pipe array in substrate using chemical vapour deposition technique, carbon nano pipe array is often attached to
On substrate surface, it is not easy to separate with growth substrate.It generallys use the tools such as a blade or tweezers and passes through mechanical external force for carbon nanometer
Pipe array peels off from the substrate, however since the adhesive force between carbon nano pipe array and substrate is larger, pass through above-mentioned mechanical stripping
Contain more catalyst granules in the carbon nano pipe array isolated from method, the quality and application for influencing carbon nanotube produce
The using effect of product.
Summary of the invention
It is necessory to provide a kind of method that carbon nano pipe array is separated with growth substrate, this method can simply, conveniently
Ground separates carbon nano pipe array with its growth substrate, and containing less or without containing urging in isolated carbon nano pipe array
Catalyst particles.
A kind of method that carbon nano pipe array is separated with growth substrate, specifically includes the following steps: provide all one's life with
Carbon nano pipe array substrate；The substrate is heated, and is passed through oxygen or oxygenous mixed gas, makes the carbon nanotube
Array is reacted with oxygen；Separate the carbon nano pipe array and substrate.
Compared with prior art, the method that carbon nano pipe array provided by the invention is separated with growth substrate makes carbon nanometer
Pipe display is reacted with oxygen, under high temperature environment, compared with the top of carbon nano pipe array and side wall, is lacked in carbon nano pipe array
It falls into more root to be easier to react with oxygen, carbon dioxide is generated, to reduce between carbon nano pipe array and substrate
Contact force separates carbon nano pipe array with its growth substrate, contains less in isolated carbon nano pipe array or is free of
There is catalyst granules, method is simple, scale and industrialization can be achieved.
Detailed description of the invention
Fig. 1 is the flow diagram for the method that carbon nano pipe array provided by the invention is separated with growth substrate.
Following specific embodiment will further illustrate the present invention in conjunction with above-mentioned attached drawing.
Specific embodiment
The preparation side of carbon nanotube provided by the technical program is described in detail below with reference to drawings and the specific embodiments
Method.
Referring to Fig. 1, the technical program provides a kind of method that carbon nano pipe array is separated with growth substrate, it is specific to wrap
Include following steps:
Step 1: substrate of all one's life with carbon nano pipe array is provided.
In the present embodiment, carbon nano pipe array is grown using chemical vapour deposition technique, specifically includes the following steps:
Firstly, providing a substrate with smooth surface.The substrate of offer is wanted high temperature resistant and is not passed through with subsequent step
Gas occur chemical reaction and atom permeate phenomena such as, the material of substrate can be silicon, quartz plate etc..Preferably, silicon base
Surface forms a protective layer, such as thin layer of silicon oxide, and thickness is generally 1~1000 nanometer (nm).The substrate surface can pass through
The methods of mechanical polishing, electrochemical polish processing, to guarantee it smoothly with the needs of Adaptable growth carbon nano pipe array.The base
The shape at bottom and size are unlimited, and shape can be plate shaped, curved form or other shapes, size can be 4 inches, 8 inches or
12 inches etc..
Secondly, depositing a catalyst layer in the substrate surface.It can be existed by vapor deposition, sputter or the method for chemical deposition
The substrate surface forms a catalyst layer, and the material of catalyst layer can be iron (Fe), cobalt (Co), nickel (Ni) or its any group
One of alloy of conjunction.Catalyst layer with a thickness of 1~10nm, preferably 1~5nm.Then, under air atmosphere, 200~400
Under degree Celsius (DEG C), the annealing of 8~12 hours (h) is carried out to catalyst, the catalyst film of substrate surface is made to become equal
The catalyst nano-particles of even distribution, to improve the catalytic activity of catalyst.
Finally, the substrate that surface is deposited with catalyst is put into a reacting furnace, in the environment of protective gas, institute is heated
Substrate is stated to 600~720 DEG C, preferably 620~700 DEG C, then passes to the mixed gas of carbon source gas and protective gas, the carbon
Source gas can be acetylene, ethylene, methane, ethane etc., and the protective gas is inert gas or nitrogen, react 10~40 minutes
(min), it grows to obtain carbon nano pipe array in the substrate surface using chemical vapour deposition technique.
Step 2: heating the substrate, and be passed through oxygen, reacts the carbon nano pipe array with oxygen.
During this, maintaining the air pressure of environment is 2~8 supports (Torr).
There are two types of the modes for heating substrate: first, the substrate for having carbon nano pipe array that grows is placed on a reacting furnace
It is interior, furnace inner environment is heated by reacting furnace and heats the substrate；Second, thering is the substrate of carbon nano pipe array to be placed on the growth
In one sealing ventilation equipment, the substrate is heated using an area heating installation, the area heating installation can be electrothermal resistance
The substrate specifically can be placed on institute by silk, coreless induction furnace, laser heating device or carbon nanotube electric heating device etc.
It states on the pedestal in sealing ventilation equipment, base-plates surface, which is equipped with below electrothermal resistance silk or carbon nanotube or pedestal, is equipped with height
Frequency furnace or laser heating device.
The substrate is heated to 500~800 DEG C, the flow for being passed through oxygen is 300~500 standard milliliters/minute (sccm),
The carbon nano pipe array reacts 5~20min with oxygen.It is appreciated that pure oxygen can be passed through, can also be passed through oxygen-containing
The mixed gas of gas, such as the mixed gas of air or oxygen and other gases.
In the present embodiment, the substrate is placed in a reacting furnace, heats the substrate to 700 DEG C, the flow of oxygen is
500sccm makes the carbon nano pipe array react 9~10min with oxygen.In certain embodiments, step 2 specifically includes: will
The substrate is placed in a reacting furnace, heats the substrate to 800 degrees Celsius, the flow of oxygen is 300sccm, the carbon nanometer
Pipe array reacts 5~7min with oxygen.In another embodiment, step 2 specifically includes: the substrate is placed on a reaction
In furnace, the substrate is heated to 500 degrees Celsius, the flow of oxygen is 500sccm, and the carbon nano pipe array reacts 16 with oxygen
~20min.
In carbon nano pipe array growth course, the top of carbon nanotube grows out at first, and the root of carbon nanotube is most
After grow, at later stages, the catalytic activity of catalyst declines, and leads to the carbon nanotube root and carbon nanotube top of late growth
Compare that there are more defects with side wall in end；Under high temperature environment, the top of oxygen and carbon nanotube, side wall and root can occur
Reaction, but compared with carbon nanotube top and side wall, the defect of carbon nanotube root is more, therefore oxygen is easier to react with root,
It generates carbon dioxide (CO2), so that carbon nano pipe array is separated with its growth substrate；And the side wall of carbon nanotube is cleaner, scarce
It falls into less, reacts less with oxygen within the measured response time or do not reacted with oxygen, so as to keep carbon nano pipe array
Integrality.
These three parameter values of the flow of the reaction temperature of the carbon nano pipe array and oxygen, reaction time and oxygen with mention
The quality of the carbon nano pipe array of confession is related, when the quality of the carbon nano pipe array of offer is lower, such as carbon nanotube
When containing more defect and amorphous carbon in array, reaction temperature can be suitably reduced, shorten the reaction time or reduces oxygen
Flow；When the quality of the carbon nano pipe array of offer is higher, such as carbon nano-pipe array is classified as and is substantially free of impurity
Super in-line arrangement carbon nano pipe array when, can properly increase reaction temperature, extend the reaction time or increase oxygen flow.
It is appreciated that when one timing of flow of reaction temperature and oxygen, the carbon nano pipe array reacted with oxygen when
Between can not be too long, when the reaction time is too long, carbon nano pipe array is impaired serious, and height will greatly reduce；The carbon nanotube
The time that array is reacted with oxygen also can not be too short, when the reaction time is too short, when carbon nano pipe array and oxygen are catalytic
Between it is few, cause the carbon nano pipe array to be not easy to separate with growth substrate.
Step 3 separates the carbon nano pipe array and substrate.
After the carbon nano pipe array reacts a period of time with oxygen, stopping is passed through oxygen, continues to be passed through protective gas, this
When can increase the circulation of protective gas, so that the temperature of the substrate is down to 350 DEG C naturally hereinafter, simply mechanical vibration at this time
It is dynamic such as to shake gently substrate, the carbon nano pipe array and the substrate natural separation can be made.Carbon nano pipe array is from close
The root of substrate is separated with substrate, and catalyst stays in substrate surface, containing seldom in the carbon nano pipe array separated with substrate
Or catalyst metal particles are not contained.
The method that a kind of carbon nano pipe array provided by the invention is separated with growth substrate has the advantage that first, logical
Enter oxygen, react carbon nano pipe array with oxygen, the root that oxygen is easier the carbon nano pipe array more with defect is reacted
Carbon dioxide is generated, so that carbon nano pipe array be made to separate with growth substrate；Second, after oxygen is reacted with carbon nano pipe array,
Carbon nano pipe array is separated from root with substrate, and catalyst can stay in substrate surface, and the carbon nano pipe array separated with substrate
In containing seldom or do not contain catalyst granules, improve the quality of carbon nanotube；Third, the carbon nano pipe array and growth base
The method of bottom separation is simple, scale and industrialization can be achieved, and is conducive to the large-scale application of carbon nanotube industrially.
In addition, those skilled in the art can also do other variations in spirit of that invention, certainly, these are smart according to the present invention
The variation that mind is done should be all included in scope of the present invention.
Claims (10)
1. a kind of method that carbon nano pipe array is separated with growth substrate comprising following steps:
Substrate of all one's life with carbon nano pipe array is provided；
The substrate is heated, and is passed through oxygen or oxygenous mixed gas, reacts the carbon nano pipe array with oxygen；
Separate the carbon nano pipe array and substrate.
2. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the carbon nanometer
The temperature that pipe array is reacted with oxygen is 500~800 degrees Celsius.
3. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the oxygen
Flow is 300~500 standard milliliters/minute.
4. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the carbon nanometer
Pipe array reacts 5~20 minutes with oxygen.
5. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the oxygen with
The root reaction of the carbon nano pipe array generates carbon dioxide.
6. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the separation institute
The step of stating carbon nano pipe array and substrate includes: that mechanical oscillation make the carbon nano pipe array and growth substrate natural separation.
7. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, which is characterized in that the heating institute
The step of stating substrate includes: that the substrate is placed in a reacting furnace, heats furnace inner environment by reacting furnace to heat the base
Bottom.
8. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate, is characterized in that, described in the heating
The step of substrate includes: that the substrate is placed in a sealing ventilation equipment, and the base is heated using an area heating installation
Bottom.
9. the method that carbon nano pipe array as claimed in claim 8 is separated with growth substrate, which is characterized in that the part adds
Hot charging is set to the group of one or more of electrothermal resistance silk, coreless induction furnace, laser heating device or carbon nanotube electric heating device
It closes.
10. the method that carbon nano pipe array as described in claim 1 is separated with growth substrate,
It is characterized in that, the air pressure of environment is maintained 2~8 supports in the carbon nano pipe array and oxygen reaction process.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423271.1A CN108996487B (en) | 2017-06-07 | 2017-06-07 | Method for separating carbon nano tube array from growth substrate |
| TW106120439A TWI688544B (en) | 2017-06-07 | 2017-06-19 | A method for separating a carbon nanotube array from its growth substrate |
| US15/990,938 US10562774B2 (en) | 2017-06-07 | 2018-05-29 | Method for separating carbon nanotube array from growth substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710423271.1A CN108996487B (en) | 2017-06-07 | 2017-06-07 | Method for separating carbon nano tube array from growth substrate |
Publications (2)
| Publication Number | Publication Date |
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| CN108996487A true CN108996487A (en) | 2018-12-14 |
| CN108996487B CN108996487B (en) | 2021-01-26 |
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| CN201710423271.1A Active CN108996487B (en) | 2017-06-07 | 2017-06-07 | Method for separating carbon nano tube array from growth substrate |
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|---|---|
| US (1) | US10562774B2 (en) |
| CN (1) | CN108996487B (en) |
| TW (1) | TWI688544B (en) |
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| CN111128637B (en) * | 2018-11-01 | 2021-02-26 | 清华大学 | Method for producing field emitters |
| CN111115615B (en) * | 2018-11-01 | 2021-08-31 | 清华大学 | Transfer method of carbon nano tube array |
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2017
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Also Published As
| Publication number | Publication date |
|---|---|
| CN108996487B (en) | 2021-01-26 |
| TW201902817A (en) | 2019-01-16 |
| US10562774B2 (en) | 2020-02-18 |
| TWI688544B (en) | 2020-03-21 |
| US20180354802A1 (en) | 2018-12-13 |
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